CN106566279A - Suaeda salsa seed haematochrome extraction process - Google Patents
Suaeda salsa seed haematochrome extraction process Download PDFInfo
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- CN106566279A CN106566279A CN201610992496.4A CN201610992496A CN106566279A CN 106566279 A CN106566279 A CN 106566279A CN 201610992496 A CN201610992496 A CN 201610992496A CN 106566279 A CN106566279 A CN 106566279A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B61/00—Dyes of natural origin prepared from natural sources, e.g. vegetable sources
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0096—Purification; Precipitation; Filtration
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- Medicines Containing Plant Substances (AREA)
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Abstract
The invention discloses a suaeda salsa seed haematochrome extraction process, which comprises the following steps of (1) fully grinding suaeda salsa seeds under liquid nitrogen; (2) adding acetone for pre-extracting, and filtering after pre-extracting so as to obtain residues; (3) adding a hydrochloric acid-methyl alcohol mixed solution into the residues, and leaching and extracting, wherein the leaching and extracting temperature is ranged from 55 to 65 DEG C, the leaching and extracting time is ranged from 1.2 to 1.8h, and the solid-liquid rate is (1 to 2)g:100mL; (4) repetitively leaching and extracting for 1 time, wherein the solid-liquid rate is (1 to 2)g:100mL; and (5) merging twice leached and extracted filter liquors, and drying to obtain a sample containing suaeda salsa seed haematochrome. By applying the method for extracting the suaeda salsa seed haematochrome, the materials can be acquired conveniently, the flow is simple, the operability is high, and the cost is lower; the extraction method is simple, convenient and easy to implement; and the extraction rate and the purity are higher.
Description
Technical field
The present invention relates to technical field of plant extraction, and in particular to a kind of Suaeda salsa seed red pigment extraction process.
Background technology
In global range, the salination of soil and secondary salinization phenomenon generally existing.China is to possess saline and alkaline in the world
One of more country in ground, the salination phenomenon of coastal area is particularly acute.Halophytess can be normal in salination environment
Growth promoter simultaneously completes life cycle, necessarily there is its specific salt tolerant mode.Suaeda salsa is that one kind is distributed widely in the Yellow River triangle
The annual halophytess of typical dilute salt form in continent area, its black seeds have hard Black seed coat, and such seed is being planted
Pigment accumulation can be preserved in long period, therefore Suaeda salsa black seeds kind skin in child resource storehouse in Suaeda salsa to environment
Adaptation aspect and the protection of seed aspect is had great importance.
There are some researches show, substantial amounts of Betacyanins are contained in Suaeda salsa seedling（The long spring 2007 of king）, betanidin and flower
Pigment is all much like in terms of color, absorption spectrum, but research shows that both pigments will not simultaneously exist in same plant,
It is inferred that the red pigment in Suaeda salsa seed should be Betacyanins or its derivant.Extracting Suaeda salsa leaf
Find during Betacyanins in piece, first carried in advance with methanol, other colors such as Chlorophylls and Carotenoids in material can be removed
Element, such that it is able to improve Aqueous extracts in Betacyanins extraction efficiency, the maximum light absorption of extracting solution is 536 nm.Barrera
The use of volume ratio is 99 Deng (1998):1 ethanol-hydrogen chloride solvent extraction Radix et Caulis Opuntiae Dillenii (Myrtillocactus
Geometrizans the Betacyanins in), find its stability not as good as Aqua pure extract liquid.Carry out in extraction process at of short duration heat
Reason (70 DEG C, 2 min) can make enzymatic degradation, or appropriate acidifying lixiviating solution precipitate can Betacyanins, steady so as to strengthen its
Qualitative (Delgado-Vargas et al., 2000).But to the extraction of red pigment in Suaeda salsa seed so far there are no report
Road.Therefore, a kind of high Suaeda salsa seed red pigment extraction process method of extraction ratio is needed badly at present.
The content of the invention
For prior art, the invention provides a kind of Suaeda salsa seed red pigment extraction process, the extraction process side
The red pigment effect that method is extracted in Suaeda salsa seed is obvious, and method is effective.
The technical solution used in the present invention is as follows：
A kind of Suaeda salsa seed red pigment extraction process, comprises the following steps：
（1）Suaeda salsa seed is fully ground under liquid nitrogen；
（2）Add acetone to carry in advance, residue is filtrated to get after carrying in advance, the temperature that acetone is carried in advance is 25 ~ 35 DEG C, the time is 40 ~ 80
min。
（3）Add in residue and extracted in hydrochloric acid-methanol mixed solution, extraction temperature is 55 ~ 65 DEG C, during extraction
Between be 1.2 ~ 1.8 h, solid-liquid ratio is（1~2）g：100 mL；
（4）Repeat extraction 1 time, solid-liquid ratio is（1~2）g：100 mL；
（5）Merging extracts twice filtrate, is dried, you can obtain the sample containing Suaeda salsa seed red pigment.
Step（1）In, the present invention chooses Suaeda salsa black seeds as raw material.Redness in Suaeda salsa black seeds
Plain accumulation is big, but melanospermous cell tissue close structure, and with other materials more stable material is combined to form, and extracts
Red pigment is not easy to.There is vital impact on extraction efficiency on the pretreatment process of specific extraction object, this will be certainly
The size of fixed last extraction ratio.Using liquid nitrogen grinding, can fully by Suaeda salsa seed grind into powder, preferably by material
Red pigment in material is extracted.Compare through same method for distinguishing, the method extraction efficiency highest.
Step（2）In, the present invention is carried in advance using acetone, can remove other pigments in Suaeda salsa, such as carotenoids
Element etc., the red pigment purity for obtaining extraction is higher, and the quality of Suaeda salsa seed is 1 g with the ratio of the volume of acetone：25~35
ML, preferably 1 g:30 mL.Preferably, the temperature that acetone is carried in advance is 30 DEG C, and the time is 1 h.Through verification experimental verification and point
Analysis, when the pre- temperature raising degree of acetone is 30 DEG C and the time is 1 h, the extraction effect of red pigment is best.
Step（3）In, different digestion agents have different impacts to extracting for red pigment, and the present invention is directed to Suaeda salsa
Seed this extracting object, hydrochloric acid and methanol mixed solution have been obtained as saline land alkali from screening and optimizing in substantial amounts of organic solvent
The digestion agent of fluffy seed, the extracting effect using this digestion agent is excellent.Through lot of experiment validation and analysis, the hydrochloric acid and
In methanol mixed solution, the volume fraction of the hydrochloric acid is 2 ~ 8%, it is preferred that the volume fraction of hydrochloric acid is 5%.
The impact of the efficiency that extraction temperature and extraction time extract red pigment to Suaeda salsa seed is larger, in order that red
The extraction efficiency of element is higher, and the extraction temperature is 60 DEG C, and extraction time is 1.5 h, extraction efficiency now and other temperature
Compare with the time, effect is projected, significant difference.
The solid-liquid ratio is the quality of residue and the ratio of the volume of hydrochloric acid-methanol mixed solution, and the solid-liquid ratio is to extraction
The content of red pigment has material impact, through substantial amounts of experimental verification and analysis, solid-liquid ratio is arranged on（1~2）g：100 mL
When, the extraction ratio of red pigment is higher, and experiment is proved when solid-liquid ratio is more than 2：100 and less than 1：When 100, the extraction ratio of red pigment is equal
It is relatively low.Preferably, the solid-liquid ratio is 1 g：100 mL, the extraction ratio of red pigment is optimal.
The present invention also protects the Suaeda salsa seed red pigment that described technique is prepared.
Above-mentioned technical proposal has the advantages that：
（1）Suaeda salsa is being capable of the heavy salinized aerial that can not be grown in crops and a kind of salt that can complete life cycle
Plant, while salt-soda soil can be improved by absorbing substantial amounts of salinity, is referred to as " pionner " in salt-soda soil, and its
Hip number is big, if it is possible to a large amount of from Suaeda salsa seed to extract red pigment, for grocery trade and commercial production, saline land alkali
Undoubtedly one kind is good material to fluffy seed, it is also possible to reach more preferably improvement and using the purpose in salt-soda soil.
（2）Compared with the nutrition organs of plant, the pigment in Suaeda salsa seed typically can be formed Suaeda salsa seed
A kind of more stable structure of matter（Play a part of to protect plant seed until sprouting）, therefore want from Suaeda salsa seed
Middle extraction pigment, it is necessary to fully crush seed material, farthest this pigment separated out, present invention employs liquid nitrogen
Under the conditions of the method that is fully ground, this can extract the key technology means of red pigment for the present invention from Suaeda salsa seed.
After another key technology means-carried in advance using acetone, can other pigments be advance carotenoid in seed etc.
Extract and red pigment is preferably dissolved, can thus remove other pigments in Suaeda salsa, make what extraction was obtained
The yield and purity of red pigment is higher.
The Extraction technique of raw material, such as solid-liquid ratio, the species of digestion agent and ratio, extraction temperature, extraction time and
Extraction temperature is also extremely important, and the present invention has obtained preferably extracting the work of red pigment in Suaeda salsa seed through screening and optimizing
Skill, the extraction ratio of the red pigment extracted by the special process is higher.And carried from Leaves of Suaeda Salsa and stem using conventional
Take the red pigment that the method for Suaeda salsa Betacyanins cannot be obtained in Suaeda salsa seed.
（3）With Suaeda salsa black seeds as raw material, research obtains a kind of rapidly and effectively red pigment and extracts the present invention
Method, provides for red pigment in the melanospermous deep processing of Suaeda salsa and recycling and scale extraction Suaeda salsa seed
Experiment basis, while providing premise to analyze the species of Suaeda salsa seed red pigment, 26S Proteasome Structure and Function.
The red pigment in Suaeda salsa seed is extracted with the method, is drawn materials conveniently, flow process is simple, strong operability, cost
Relatively low, the extracting method is the most simple and easy to do, and extraction ratio and purity are higher, and extraction ratio is 96.4%, and it is 356.83 to extract yield
mg kg-1 DW。
（4）Content of the present invention also for red pigment in discussion seed establishes base with adaptation sexual intercourse of the Suaeda salsa seed to environment
Plinth, is that red pigment is offered reference in industry, during grocery trade extracts on a large scale Suaeda salsa seed, and to study Suaeda salsa seed
The species of middle red pigment, structure, function, application and ecological significance lay the foundation.
Description of the drawings
Fig. 1：Different feed liquid compares the impact of red cellulose content in Suaeda salsa black seeds.
Fig. 2：Acetone proposes in advance the impact to red cellulose content in Suaeda salsa black seeds.
Fig. 3：Impact of the different hydrochloric acid/methanol ratios to red cellulose content in Suaeda salsa black seeds.
Fig. 4：Impact of the different extraction temperatures to red cellulose content in Suaeda salsa black seeds.
Fig. 5：Impact of the different extraction times to red cellulose content in Suaeda salsa black seeds.
Fig. 6：Impact of the different extracting times to red cellulose content in Suaeda salsa black seeds.
Specific embodiment
With reference to embodiment, the present invention is further described.
Embodiment 1
A kind of Suaeda salsa seed red pigment extraction process, comprises the following steps：
1）The g of Suaeda salsa black seeds 0.1 is weighed respectively, in mortar, is fully ground under liquid nitrogen.
2）Plus 3 the acetone of mL carry in advance, the temperature for carrying in advance is 30 DEG C, and the time is 1 h.
3）5 mL volume fractions are added to be 5% hydrochloric acid-methanol solution in residue.
4）1.5 h are extracted in 60 DEG C of water-baths, and control solid-liquid ratio is respectively 1 g：100 mL.
5）Repeat water-bath to extract 1 time, with step（4）In solid-liquid ratio arrange it is identical.
6）Merging filtrate, is dried to obtain the sample containing Suaeda salsa seed red pigment.
When determining red cellulose content, step 6）：Merging filtrate is simultaneously settled to 10 mL, you can farthest obtain saline land
Red cellulose content in Herba suadeae glaucae black seeds.
Embodiment 2
A kind of Suaeda salsa seed red pigment extraction process, comprises the following steps：
1）The g of Suaeda salsa black seeds 0.1 is weighed respectively, in mortar, is fully ground under liquid nitrogen.
2）Plus 2.8 the acetone of mL carry in advance, the temperature for carrying in advance is 30 DEG C, and the time is 1 h.
3）5 mL volume fractions are added to be 4.5% hydrochloric acid-methanol solution in residue.
4）1.6 h are extracted in 55 DEG C of water-baths, and control solid-liquid ratio is respectively 1 g：100 mL、3 g：100 mL、5 g：100
mL、7 g：100 mL.
5）Repeat water-bath to extract 1 time, with step（4）In solid-liquid ratio arrange it is identical.
6）Merging filtrate, is dried to obtain the sample containing Suaeda salsa seed red pigment, and different feed liquid compares Suaeda salsa
Fig. 1 is shown in the impact of red cellulose content in black seeds.
Embodiment 3
A kind of Suaeda salsa seed red pigment extraction process, comprises the following steps：
1）The g of Suaeda salsa black seeds 0.1 is weighed respectively, in mortar, is fully ground under liquid nitrogen.
2）Plus 2.8 the acetone of mL carry in advance, the temperature that acetone is carried in advance is 30 DEG C, and the time is 1 h.
3）5 mL volume fractions are added to be 4.5% hydrochloric acid-methanol solution in residue.
4）1.6 h are extracted in 55 DEG C of water-baths, and control solid-liquid ratio is respectively 1.5 g：100 mL.
5）Repeat water-bath to extract 1 time, with step（4）In solid-liquid ratio arrange it is identical.
6）Merging filtrate, is dried to obtain the sample containing Suaeda salsa seed red pigment.
Comparative example is set, by the step 2 in embodiment 2）Acetone carry in advance step deletion.Acetone is carried in advance to saline land alkali
Fig. 2 is shown in the impact of red cellulose content in fluffy black seeds.
Embodiment 4
A kind of Suaeda salsa seed red pigment extraction process, comprises the following steps：
1）The g of Suaeda salsa black seeds 0.1 is weighed respectively, in mortar, is fully ground under liquid nitrogen.
2）Plus 2.8 the acetone of mL carry in advance, the temperature for carrying in advance is 30 DEG C, and the time is 1 h.
3）5 mL volume fractions are separately added into in residue for 1%, 5%, 10% and 15% hydrochloric acid-methanol solution.
4）1.6 h are extracted in 55 DEG C of water-baths, and control solid-liquid ratio is respectively 1.5 g：100 mL.
5）Repeat water-bath to extract 1 time, with step（4）In solid-liquid ratio arrange it is identical.
6）Merging filtrate, is dried to obtain the sample containing Suaeda salsa seed red pigment, and different hydrochloric acid/methanol ratios are to salt
Fig. 3 is shown in the impact of red cellulose content in ground Herba suadeae glaucae black seeds.
Embodiment 5
A kind of Suaeda salsa seed red pigment extraction process, comprises the following steps：
1）The g of Suaeda salsa black seeds 0.1 is weighed respectively, in mortar, is fully ground under liquid nitrogen.
2）Plus 2.8 the acetone of mL carry in advance, the temperature for carrying in advance is 30 DEG C, and the time is 1 h.
3）5 mL volume fractions are separately added into in residue for 4.5% hydrochloric acid-methanol solution.
4）Respectively in room temperature（25 ℃）, 40 DEG C and 60 DEG C of water-baths extract 1.6 h, control solid-liquid ratio is respectively 1.5 g：
100 mL。
5）Repeat water-bath to extract 1 time, with step（4）In solid-liquid ratio arrange it is identical.
6）Merging filtrate, is dried to obtain the sample containing Suaeda salsa seed red pigment, and different extraction temperatures are to saline land alkali
Fig. 4 is shown in the impact of red cellulose content in fluffy black seeds.
Embodiment 6
A kind of Suaeda salsa seed red pigment extraction process, comprises the following steps：
1）The g of Suaeda salsa black seeds 0.1 is weighed respectively, in mortar, is fully ground under liquid nitrogen.
2）Plus 2.8 the acetone of mL carry in advance, the temperature for carrying in advance is 30 DEG C, and the time is 1 h.
3）5 mL volume fractions are separately added into in residue for 4.5% hydrochloric acid-methanol solution.
4）0.5 h, 1 h, 1.5 h and 2 h are extracted respectively using 55 DEG C of water-baths, and control solid-liquid ratio is respectively 1.5 g：100
mL。
5）Repeat water-bath to extract 1 time, with step（4）In solid-liquid ratio arrange it is identical.
6）Merging filtrate, is dried to obtain the sample containing Suaeda salsa seed red pigment, and different extraction times are to saline land alkali
Fig. 5 is shown in the impact of red cellulose content in fluffy black seeds.
Embodiment 7
A kind of Suaeda salsa seed red pigment extraction process, comprises the following steps：
1）The g of Suaeda salsa black seeds 0.1 is weighed respectively, in mortar, is fully ground under liquid nitrogen.
2）Plus 2.8 the acetone of mL carry in advance, the temperature for carrying in advance is 30 DEG C, and the time is 1 h.
3）5 mL volume fractions are separately added into in residue for 4.5% hydrochloric acid-methanol solution.
4）1.6 h are extracted respectively using 55 DEG C of water-baths, and control solid-liquid ratio is respectively 1.5 g：100 mL.
5）Repeat water-bath respectively to extract 1 time, 2 times and 3 times, with step（4）In solid-liquid ratio arrange it is identical.
6）Merging filtrate, is dried to obtain the sample containing Suaeda salsa seed red pigment, and different extracting times are to saline land alkali
Fig. 6 is shown in the impact of red cellulose content in fluffy black seeds.In theory, leaching number of times is more, and the red pigment dissolution in sample is more,
Extraction ratio more levels off to a certain steady state value, but red pigment extraction ratio continuing to increase and reduce on the contrary with extraction time in the present invention,
Extraction time reaches highest extraction ratio for 2 times, and extraction ratio does not increase with the increase of extraction time, and this is mainly due to reality
Operation during testing is caused, because extraction time is more, the operation such as transfer, merging increases, and extract loss is also larger, while carrying
Take that the time is also corresponding long, therefore 2 i.e. available higher red pigment extraction ratios are extracted in water-bath of the present invention.
By extracting red pigment content balance (Fig. 1-6) in Suaeda salsa black seeds with different process method, can
To find out, the g of Suaeda salsa seed 0.1, as extraction solvent, solid-liquid ratio is 1 to the hydrochloric acid-methanol with 5%:100, through 30 DEG C third
Ketone is carried in advance after 1h, and 60 DEG C of water-baths are extracted twice, every time 1.5 h, and filtration is settled to 10 mL, and light absorbs are determined at 536 nm, can
The more stable seed red pigment of maximum, property is obtained, is optimized extracting method as described in Example 1.Can by Fig. 1-6
To find out, the red pigment effect extracted using the process for extracting in Suaeda salsa seed is obvious, and effectively, extraction ratio is method
96.4%, extraction yield is 356.83 mg kg-1DW, extracts yield（mg kg-1DW）The extraction of red pigment in=optimised process
Amount（mg）The dry weight of/material（kg）.
Above-described embodiment is the present invention preferably embodiment, but embodiments of the present invention not by above-described embodiment
Limit, other any spirit without departing from the present invention and the change, modification, replacement made under principle, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (10)
1. a kind of Suaeda salsa seed red pigment extraction process, is characterized in that, comprise the following steps：
（1）Suaeda salsa seed is fully ground under liquid nitrogen；
（2）Add acetone to carry in advance, residue is filtrated to get after carrying in advance, the temperature that acetone is carried in advance is 25 ~ 35 DEG C, the time is 40 ~ 80
min；
（3）Add in residue and extracted in hydrochloric acid-methanol mixed solution, extraction temperature is 55 ~ 65 DEG C, extraction time is
1.2 ~ 1.8 h, solid-liquid ratio is（1~2）g：100 mL；
（4）Repeat extraction 1 time, solid-liquid ratio is（1~2）g：100 mL；
（5）Merging extracts twice filtrate, is dried, you can obtain the sample containing Suaeda salsa seed red pigment.
2. technique as claimed in claim 1, is characterized in that：Step（1）In, the Suaeda salsa seed is black seeds.
3. technique as claimed in claim 1, is characterized in that：Step（2）In, the quality of Suaeda salsa seed and the body of acetone
The ratio of product is 1 g：25~35 mL.
4. technique as claimed in claim 3, is characterized in that：The quality of Suaeda salsa seed is 1 with the ratio of the volume of acetone
g:30 mL。
5. technique as claimed in claim 1, is characterized in that：Step（2）In, the temperature for carrying in advance is 30 DEG C.
6. technique as claimed in claim 5, is characterized in that：Step（2）In, the time for carrying in advance is 1 h.
7. technique as claimed in claim 1, is characterized in that：Step（3）In, it is described in the hydrochloric acid and methanol mixed solution
The volume fraction of hydrochloric acid is 2 ~ 8%.
8. technique as claimed in claim 7, is characterized in that：The volume fraction of the hydrochloric acid is 5%.
9. technique as claimed in claim 1, is characterized in that：Step（4）In, the extraction temperature is 60 DEG C, and extraction time is
1.5 h。
10. the sample containing Suaeda salsa seed red pigment for being prepared using the technique any one of claim 1 ~ 9
Product.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101204217A (en) * | 2007-12-20 | 2008-06-25 | 山东师范大学 | Method for extracting beet red pigment from Suaeda salsa |
| CN101747663A (en) * | 2010-01-18 | 2010-06-23 | 山东理工大学 | Method for producing betanine with suaeda salsa seed |
| CN102653634A (en) * | 2011-03-02 | 2012-09-05 | 盐城工学院 | Ultrasound-assisted method for extracting betacyanin from suaeda salsa |
-
2016
- 2016-11-10 CN CN201610992496.4A patent/CN106566279A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101204217A (en) * | 2007-12-20 | 2008-06-25 | 山东师范大学 | Method for extracting beet red pigment from Suaeda salsa |
| CN101747663A (en) * | 2010-01-18 | 2010-06-23 | 山东理工大学 | Method for producing betanine with suaeda salsa seed |
| CN102653634A (en) * | 2011-03-02 | 2012-09-05 | 盐城工学院 | Ultrasound-assisted method for extracting betacyanin from suaeda salsa |
Non-Patent Citations (1)
| Title |
|---|
| 王长泉: "盐地碱蓬甜菜红素的鉴定及其生物合成的生理机制研究", 《中国博士学位论文全文数据库 基础科学辑》 * |
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